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Preparation method of mesoporous nickel cobaltate fiber and application thereof

A technology of nickel cobalt oxide and fiber, applied in the field of preparation of nickel cobalt oxide, can solve the problems of low product purity, small specific surface area, low catalytic activity, etc., and achieve the effects of high purity, large specific surface area, and high specific surface area.

Active Publication Date: 2013-09-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, in an oxygen atmosphere, the precursor needs to be thermally decomposed at a temperature of about 500°C to obtain fibrous porous nickel cobaltate. According to the properties of nickel cobaltate itself, this kind of nickel cobaltate product has low purity, small specific surface area, and catalytic activity. low energy consumption

Method used

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  • Preparation method of mesoporous nickel cobaltate fiber and application thereof
  • Preparation method of mesoporous nickel cobaltate fiber and application thereof
  • Preparation method of mesoporous nickel cobaltate fiber and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Weigh 0.02mol of NiCl with a purity of 98.0% respectively 2 ·6H 2 O and 0.04 mol purity of 99.0% CoCl 2 ·6H 2 O, NiCl 2 ·6H 2 O and CoCl 2 ·6H 2 The ratio of the amount of O substance is 1:2. NiCl 2 ·6H 2 O and CoC l2 ·6H 2 O was co-dissolved in 100ml deionized water and formulated to contain Ni 2+ and Co 2+ The mixed metal salt solution A100ml, the mixed metal salt solution A, Ni 2+ and Co 2+ The total concentration is 0.6mol / L.

[0040] 2) Dissolve 0.072mol of oxalic acid with a purity of 99% in a mixed solvent of 50ml of organic reagent ethanol and 50ml of deionized water. The organic reagent is ethanol with a purity of 99.7%, and configure it as oxalic acid solution B.

[0041] 3) Add 100ml of mixed metal salt solution A prepared in step 1 dropwise to 100ml of oxalic acid solution B prepared in step 2, stir while adding dropwise, while controlling the reaction temperature to 60°C, adjust the pH value with ammonia water, and keep the pH value 8.2, ...

Embodiment 2

[0045] Example 2: Electrode material prepared by mesoporous nickel cobaltate and its electrochemical characterization

[0046] A modified glassy carbon electrode was used as the working electrode. First, use 50nm alumina polishing powder to grind the glassy carbon electrode on a polishing cloth until the surface is smooth; then ultrasonically wash it three times in distilled water, and dry it for use. Take 0.05 g of the mesoporous nickel cobaltate powder prepared in Step Example 1, dissolve it in 2 mL of distilled water, and disperse evenly by ultrasonic; use a micro-sampler to draw 0.4 μL of sample, and apply it on the surface of the glassy carbon electrode. After drying at room temperature, 0.2 μL of Nafion solution (0.5 wt%) was applied to the surface of the sample. After drying at room temperature, a glassy carbon electrode modified with mesoporous nickel cobaltate was obtained, with a loading capacity of 0.5 mg / cm 2 .

[0047] The glassy carbon electrode modified by me...

Embodiment 3

[0051] 1) Weigh 0.02mol of NiCl with a purity of 98.0% respectively 2 ·6H 2 O and 0.04 mol purity of 99.0% CoCl 2 ·6H 2 O, the NiCl 2 ·6H 2 O and CoCl 2 ·6H 2 The ratio of the amount of O substance is 1:2. The NiCl 2 ·6H 2 O and CoCl 2 ·6H 2O, dissolved together in 100ml deionized water, formulated to contain Ni 2+ and Co 2+ 100ml of mixed metal salt solution A, the mixed metal salt solution A, Ni 2+ and Co 2+ The total concentration is 0.6mol / L.

[0052] 2) Dissolve 0.072mol of ammonium oxalate with a purity of 99.0% in a mixed solvent of 20ml of ethanol and 80ml of deionized water, the ethanol is ethanol with a purity of 99.7%, and configure as oxalate solution B.

[0053] 3) Add 100ml of mixed metal salt solution A prepared in step 1 dropwise to 100ml of oxalic acid solution B prepared in step 2), stir while adding dropwise, while controlling the reaction temperature to 60°C, adjust the pH value with ammonia water, and maintain the pH value is 8.0, after the...

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Abstract

The invention brings forward a preparation method of mesoporous nickel cobaltate fiber. According to the preparation method, an organic solvent is added during the preparation process of a precursor; a mixed phase of a water phase and an organic phase is used as a solvent, soluble nickel salt and cobalt salt are used as raw materials, and oxalate is used as a precipitating agent; in a system of Ni<2+>-Co<2+>-NH3-NH4<+>-SG<n->-C2O4<2->-H20-C2H5OH, a fibrous precursor is prepared; and the fibrous precursor is subjected to thermal decomposition in the air atmosphere at 250-400 DEG C so as to obtain the mesoporous NiCo2O4 fiber. According to the invention, coprecipitation based on the Ni-Co ratio set in the raw materials is effectively realized. The prepared NiCo2O4 powder is a cubic phase, has high purity and large specific surface area, is fibrous and porous, and is applicable to be used as a catalyst or an alkaline solution oxygen-evolution / hydrogen-evolution electrode material or direct alcohol fuel cell anode catalyst. The method provided by the invention is simple to operate and easy to control, has advantages of mild condition and low cost, and is suitable for commercialized production.

Description

technical field [0001] The invention belongs to the field of one-dimensional transition metal oxides, and in particular relates to a preparation method and application of nickel cobaltate. Background technique [0002] In recent years, direct alcohol fuel cells have attracted extensive attention due to their non-toxicity and high theoretical energy density. At present, most of the anode catalysts used are platinum, ruthenium and other noble metals and their binary or multi-component materials, which are costly and prone to CO poisoning in the battery reaction. Therefore, looking for non-noble metals with good catalytic performance and low cost as an alternative anode catalyst has become There is an urgent need for the development of direct alcohol fuel cells. Nickel cobalt oxide (NiCo 2 o 4 ) is a composite oxide with an inverse spinel structure, which has excellent electrochemical properties, and its conductivity and electrochemical activity are higher than those of sing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/90
CPCY02E60/50
Inventor 湛菁张传福黎昌俊蔡梦王晨
Owner CENT SOUTH UNIV
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